HPLC法测定伪麻非索缓释胶囊中盐酸非索非那定有关物质

目的: 建立高效液相色谱法测定伪麻非索缓释胶囊中盐酸非索非那定有关物质. 方法: 方法一,采用Agilent SB-phenyl色谱柱(250 mm×4.60 mm,5 μm),以磷酸盐高氯酸缓冲液(6.64 g·L^-1磷酸二氢钠和0.84 g·L^-1高氯酸钠混合水溶液,用磷酸调节pH至2.0)-乙腈-三乙胺(650:350:3)为流动相,流速1.5 mL·min^-1,柱温30 ℃,检测波长220 nm.方法二,采用SUPELCO^® β-环糊精键合多孔硅胶填充柱Astec CYCLOBOND^TMI 2000(250 mm×4.60 mm,5 μm),以醋酸盐缓冲液(取冰醋酸2.3 mL,加水至2000 mL,用6 mol·L^-1的氢氧化铵溶液调节pH至4.0±0.1)-乙腈(85:15)为流动相,流速0.7 mL·min^-1,检测波长220 nm. 结果: 盐酸非索非那定与有关物质能有效分离,盐酸非索非那定杂质A、B、C、D的最低检测限分别为1.81、0.90、1.54、1.56 ng.杂 质A、B以加校正因子的自身对照法计算含量,校正因子分别为1.4、1.3.不加校正因子的自身对照法计算杂质C、D以及其他未知杂质的含量. 结论: 本法专属性强,简便快捷、准确灵敏,可用于该制剂的质量控制.

Objective: To develop an HPLC method for the quantitative determination of related impurities of fexofenadine hydrochloride in fexofenadine hydrochloride and pseudoephedrine hydrochloride sustained release capsules. Methods: The first method was developed by using Agilent SB-phenyl(250 mm×4.60 mm,5 μm)column.The mobile phase was composed of phosphate buffer(mixture of 0.664% sodium dihydrogen phosphate and 0.084% sodium perchlorate,pH adjusted to 2.0 with phosphoric acid)-acetonitrile-triethylamine(65:35:0.3)pumped at a flow rate of 1.5 mL·min^-1.The UV detector was operated at 220 nm,and the column temperature was 30 ℃.The second method was performed on SUPELCO^® a β-cyclodextrin bonded column Astec CYCLOBOND^TMI 2000(250 mm×4.60 mm,5 μm)with the mobile phase consisting of acetate buffer(0.115% glacial acetic acid solution,adjusted to pH 4.0±0.1 with 6 mol·L^-1 ammonia hydroxide solution)and acetonitrile(85:15),and the flow rate was 0.7 mL·min^-1.The detection wavelength was 220 nm. Results: Fexofenadine hydrochloride and related substances were effectively separated.The detection limitation of impurity A,B,C,D was 1.81 ng,0.90 ng,1.54 ng,1.56 ng,respectively.The correction factor of impurity A and B was 1.4 and 1.3,respectively.The contents of fexofenadine impurities A,B were calculated by the self contrast method with correction factor,the contents of impurities C,D and other unknown impurities were calculated by the self contrast method without correction factor. Conclusion: The method is sensitive,specific,simple and suitable for quality control of fexofenadine hydrochloride and pseudoephedrine hydrochloride sustained release capsules.